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The NanoDefiner: decision flow scheme, e-tool and manual Hubert Rauscher & Agnieszka Mech (JRC) NanoDefine Outreach Event Brussels, September 2017 NanoDefine is funded by the European Community's Seventh Framework Programme under Grant

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NanoDefine is funded by the European Community's Seventh Framework Programme under Grant Agreement-604347

The NanoDefiner: decision flow scheme, e-tool and manual

Hubert Rauscher & Agnieszka Mech (JRC)

NanoDefine Outreach Event

Brussels, September 2017

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SLIDE 2

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  • Nano or non-nano: a guided decision flow
  • Knowledge base: Performance of particle size measurement

methods

  • Matching methods and materials: Material classification system
  • The machinery: NanoDefine decision support flow scheme
  • NanoDefiner e-tool
  • How the e-tool can help regulators and clients
  • The NanoDefine Manual

Outline

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SLIDE 3

The European Commission definition of Nanomaterial

COMMISSION RECOMMENDATION of 18 October 2011 (2011/696/EU)

"Nanomaterial" means a natural, incidental or manufactured material containing particles, in an unbound state or as an aggregate or as an agglomerate and where, for 50 % or more of the particles in the number size distribution, one or more external dimensions is in the size range 1 nm - 100 nm”

The EC NM Definition

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Basic sorting Tier 1 (screening) Dispersions / Powder Tier 2 (confirmatory) Borderline? (If D50 100 nm-250 nm) yes no Decision: Nano / non-nano Decision: Nano / non-nano

Decision flow scheme - concept

  • Economic decision on nano/non-nano
  • Exit decision scheme as early as possible
  • Flexibility for the user:
  • Choice of methods
  • Tier1 / tier 2
  • Built-in priority:

Avoid false negative NMs (i.e. classification as non-NM when it actually is a NM)

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Some materials are "nano"

  • r "non-nano"

by definition Start

  

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SLIDE 5

Pillars of the decision process

Knowledge Base

  • Evaluated sizing techniques
  • Techniques performance database
  • material characteristics and templates
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Methods recommended by NanoDefine method evaluation (Babick et al. 2016)

Methods not evaluated by NanoDefine

TEM SEM BET DEMA spray AC - turb AC-RI DLS sp ICP-MS AFM

MAIN (selected) CRITERIA FOR MONOTYPE PARTICLES

CHEMICA L COMPOSIT ION Inorganic X X X X X X X X X Carbon based X X X X X X X X Organic particulate X X X X X X X X Biological X X X X X X X COMPO

  • SITE

Core shell X X X X X X1 X X X Multiple coating X X X X X1 X1 X X X Occluded X X X X X1 X1 X X X SMALL DIMENSION S 1 X X2 X X 2 X X X X 3 X X X X X X X X X Mixture X X X SHAPE Spherical or equiaxial X X X X X X X X X Elongated X X X X Flat X2 X2 X X mixture X, X3,4 X Size range (nm) 1 nm-1000 µm 10 nm - 1000 µm 1 nm -10 µm 2 nm - 1 µm 5 nm- 100 µm 1 nm – 1 µm 3 nm – 5 µm 20 nm -1 µm 1 nm -10 µm TRADE FORM Powder X3 X* X X2 Suspension X3 X3 X X X X X X2 Aerosol X Electron beam sensitive X X X X X X X Sensitivity to vacuum X X X X X X Analysis temperature (C) 15-40 15-40 15-40 10-40 5-60 5-60 5-60 15-40 15-40 Conductive materials X X X X X X X X X

Methods and their performance (selection)

Can be material dependent 6

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Knowledge Base

  • Evaluated sizing techniques
  • Techniques performance database
  • material characteristics and templates

Knowledge Base

  • Evaluated sizing

techniques

  • Techniques performance

database

  • material characteristics

and templates

Material classification system

  • method-driven
  • uses properties which determine the

suitability of a sizing technique

  • To match materials with appropriate

size measurement techniques

Pillars of the decision process

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SLIDE 8

Monotype particles Chemical composition Number of small dimensions and shape Size range Trade Form and Dispersibility Stability of particles during testing Specific properties

Material classification system

  • The material is classified according to several parameters that are most

important for size measurement methods

  • Main properties:

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Chemical composition Inorganic Carbon-based Organic, particulate Biological Other type of particles Composite Core/shell Multiple coatings Occluded particles Unknown

Material classification system

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Monotype particles Chemical composition Inorganic Carbon- based Organic, particulate Biological Other type of particles Composite Core/shell Multiple coatings Occluded particles Unknown Number of small dimensions and shape Number of small dimensions 1 2 3 Mixture of different nanoscaled materials Shape Sphere Equiaxial Elongated Flat Other/ Unknown Mixture of different shaped particles Size range Specify Trade Form and Dispersibility Trade Form Powder Suspension Aerosol Dispersibility Dispersible in aqueous media Dispersible in material- specific media and protocols Dispersible in polar media Dispersible in a non polar media Can be aerosolized Stability of particles during testing E-beam Vacuum stability Release of ions/ atoms/ molecules Heating Cooling Specific properties Electrically conductive Magnetic properties Size- dependent absorption of photons / fluorescence Functionalised

Complete material classification system for monotype particles

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More information: Poster

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Material classification system

  • method-driven
  • uses properties which

determine the suitability

  • f a sizing technique
  • To match materials with

appropriate size measurement techniques

Knowledge Base

  • Evaluated sizing

techniques

  • Techniques performance

database

  • material characteristics

and templates

Material classification system

  • method-driven
  • uses properties which determine the

suitability of a sizing technique

  • To match materials with appropriate

size measurement techniques

Decision flow scheme

  • Logical flow scheme
  • 2-tiered approach
  • screening and confirmatory methods
  • 'nano' or 'non-nano' classification

Pillars of the decision process

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SLIDE 12

NanoDefine - Decision flow scheme

  • To be published -
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SLIDE 13

Material classification system

  • method-driven
  • uses properties which

determine the suitability

  • f a sizing technique
  • To match materials with

appropriate size measurement techniques

Knowledge Base

  • Evaluated sizing

techniques

  • Techniques performance

database

  • material characteristics

and templates

Decision flow scheme

  • Logical flow scheme
  • 2-tiered approach
  • screening and

confirmatory methods

  • 'nano' or 'non-nano'

classification

Decision flow scheme

  • Logical flow scheme
  • 2-tiered approach
  • screening and confirmatory methods
  • 'nano' or 'non-nano' classification

Data input

  • Measurements/results
  • pre-evaluated EM (Nanosizer)
  • pre-evaluated sp ICP-MS

The NanoDefiner eTool

Nanomaterial No nanomaterial

Reporting

  • Dossier

Data input

  • Measurements
  • Nanosizer
  • sp ICP-MS

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Pillars of the decision process

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Material description Dossier definition Administrative data Purpose Screening method (tier 1) Data import Classification as nano Measurement technique Recommendation and selection Confirmatory method (tier 2) Data import Classification as non-nano Report generation

[Screening technique (tier 1)] [Confirmatory technique (tier 2)]

Start End

[borderline] [non-borderline] [nano] [non-nano]

E-tool flow scheme

eTool workflow

  • Dossier creation
  • Particulate material description
  • Technique selection
  • Result evaluation
  • Report generation

14

See presentation tomorrow by Christoph Friedrich

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  • Supports users who need to identify

nanomaterials, e.g., for registration purposes

  • Addressed to users with knowledge on particle

size measurements

  • Guided workflow (applied decision flow scheme)
  • Matches material properties with method

performance

  • Transparent method recommendation
  • Supports economic decisions
  • Comprehensive and transparent reporting
  • Online manual and help (in final version)
  • Configurable by expert user administrator

Summary: How the e-tool can help to identify nanomaterials

Outside of the e-tool's scope:

  • Provide details on preparation
  • Give detailed instructions on methods
  • Consider methods in development
  • Give legally valid advice
  • Provide legally valid classification
  • Substitute expert assessment

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NanoDefine Methods Manual

Objectives

  • To provide guidance to the industry,

regulators and stakeholders through the nanomaterial characterization process

  • To assists the user in choosing the

most appropriate measurement method(s) to identify/classify as nano

  • r non-nanomaterial any substance or

mixture for a specific purpose, according to the EC recommendation for a definition of nanomaterial.

  • To provide the manual for the users of

NanoDefiner e-tool

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Methods Manual

Methods description Methods evaluation Material classification scheme Decision Flow Scheme Sample preparation SOPs Metrics Conversion Information on standards

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Content

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Evaluation of the performance, characterization, application range and the limits of methods

Methods Manual

Methods description Methods evaluation Material classification scheme Decision Flow Scheme Sample preparation SOPs Metrics Conversion Information on standards

Content: Measurement methods

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Matching material properties with appropriate measurement technique

Methods Manual

Methods description Methods evaluation Material classification scheme Decision Flow Scheme Sample preparation SOPs Metrics Conversion Information on standards

Methods recommended by NanoDefine method evaluation (Babick et al. 2016)

Methods not evaluated by NanoDefin e

TEM SEM BET DEMA spray AC - turb AC-RI DLS sp ICP- MS AFM

MAIN (selected) CRITERIA FOR MONOTYPE PARTICLES

CHEMICAL COMPOSITI ON Inorganic X X X X X X X X X Carbon based X X X X X X X X Organic particulate X X X X X X X X Biological X X X X X X X COMPO- SITE Core shell X X X X X X1 X X X Multiple coating X X X X X1 X1 X X X Occluded X X X X X1 X1 X X X SMALL DIMENSIONS 1 X X2 X X 2 X X X X 3 X X X X X X X X X Mixture X X X SHAPE Spherical or equiaxial X X X X X X X X X Elongated X X X X Flat X2 X2 X X mixture X, X3,4 X Size range (nm) 1 nm-1000 µm 10 nm - 1000 µm 1 nm -10 µm 2 nm - 1 µm 5 nm- 100 µm 1 nm – 1 µm 3 nm – 5 µm 20 nm -1 µm 1 nm -10 µm TRADE FORM Powder X3 X* X X2 Suspension X3 X3 X X X X X X2 Aerosol X Electron beam sensitive X X X X X X X Sensitivity to vacuum X X X X X X Analysis temperature (C) 15-40 15-40 15-40 10-40 5-60 5-60 5-60 15-40 15-40 Conductive materials X X X X X X X X X

Content: Material Classification Scheme

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Methods Manual

Methods description Methods evaluation Material classification scheme Decision Flow Scheme Sample preparation SOPs Metrics Conversion Information on standards

NO

All existing and novel materials

Basic Classification Basic sorting of materials according to EU definition Possible nanomaterial Prioritize route (Descriptive EM/Dispersion Methods)* Nanomaterial by EU definition ( SWCNT, fullerenes, graphene) NO Nanomaterial by EU definition (non-particular materials such as proteins or micelles and nanostuctured materials) BET-Measurement Measurement as powder Measurement as dispersion Tier 1 dispersion method Tier 1 Screening Methods No Nanomaterial by EU definition Nanomaterial by EU definition E-Microscopy No Nanomaterial by EU definition Verify size with initial descriptive SEM (or go to BET if possible) Nanomaterial by EU definition Tier 2 Confirmato ry Methods

Skip tier 1

VSSA > 8/16/24

Accept X50 < 100 X50 > 100

Size OK* X50 > 250

YES YES YES Accept YES YES

No Nanomaterial by EU definition VSSA > 6

YES NO NO NO NO NO NO

Determination of shape ( descriptiveSEM)

Accept Homoge nous NO VSSA > 20/40/60 NO YES YES

X50 > 100

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*only if necessary; allows to acquire

basic knowledge on the sample

*Size OK if x50 in

dispersion is consistent below a factor 2 with a dispersion-free method such as BET

  • r descriptive EM

𝑒𝑛𝑗𝑜𝑊𝑇𝑇𝐵 𝐸 = 2𝐸 𝑊𝑇𝑇𝐵

Content: Decision Flow Scheme

Assisting in identification/classification of a material as nano or non-nanomaterial according to the EC recommendation for a definition of nanomaterial.

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Methods Manual

Methods description Methods evaluation Material classification scheme Decision Flow Scheme Sample preparation SOPs Metrics Conversion Information on standards

Content: SOPs and standards

Providing SOPs for sampling and sample preparation

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NanoDefiner e-tool

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Publicly available as JRC Technical Report stored in EC public science hub.

Where to find it?

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Summary and Outlook

  • Decision Flow Scheme, NanoDefiner e-Tool and Manual are

comprehensive tools to facilitate the regulatory identification

  • f nanomaterials
  • The tools can be adapted to changes in the regulatory

requirements

  • NanoDefiner e-Tool and Manual will be publicly available after

the end of the project

  • JRC is preparing Guidance on the implementation of the EC

definition of nanomaterials which will benefit from NanoDefine results

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Thank you!